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Author: Subject: Series of ETN nitration problems
underground
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[*] posted on 4-6-2018 at 06:12


Ok today i tried another small batch as i described above but this time i increase the temp to 35 C at the last 30 min. I did not got any yields. It looks like the safe temp, at least with this method, is somewhere between 20-35 C. I really have no idea how patents go up to some crazy temps like 40-60 C. I won't never again try to go above 20 C, i believe it doesnt worth. Next time i will try to scale it up to 200ml SA and see how it will work.
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XeonTheMGPony
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[*] posted on 4-6-2018 at 19:17


you really need to distill the acid, I had superior results with care fully distilled H2SO4. this eliminates a huge variable!
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Laboratory of Liptakov
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[*] posted on 4-6-2018 at 21:17


I have same opinion as Xeon. Undeground, You need distillation assembly. For SA and for NA. And for 100 next procedures. Both are basic compound of all researcher. Testing different temperatures are the blind way. In this problem of low yields.



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XeonTheMGPony
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[*] posted on 6-6-2018 at 04:14


Yup just no getting around some basic core glass wear, where not having it is actually dangerous to you and others.

I even care fully distill my acetone even for use as a solvent and I have found large amounts of crap after wards at time.

You need to remove variables and drain cleaner sulfuric is a big one.

Next what was the original source of the Erythritol? If pure it will be good.
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[*] posted on 6-6-2018 at 05:16


I can see your points Laboratory and Xeon but i really want to keep things as much simple as possible. Anyway i did another nitratation and the yields really shocked me, maybe i got close to 80-90%, they are still drying, i can tell you precisely after it will be completely dry. I used 400gr H2SO4 (about 219ml 98%), 120gr Kno3, 21g E (I should have use 30g but i reduced the ammount to 21g thinking that i could reduce the lower nitrated esters and looks like it worked). The procedure was exactly as Laboratory said to me. Yields looking close to 40g recrystalized. :D

[Edited on 6-6-2018 by underground]
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roXefeller
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[*] posted on 6-6-2018 at 18:22


Quote: Originally posted by underground  
I can see your points Laboratory and Xeon but i really want to keep things as much simple as possible.


If you want simple, go with acetone peroxide. Explosives aren't something we enter into looking for the simplest routes. You wouldn't jump out of an airplane with a kite just because it was easy to buy and parachutes were sold out. Get the tools, glassware, and the reagents that are necessary before jumping out the door. ETN was the very compound that started the "Life after detonation" thread.

And why are you scaling up your reaction when you're still working out the parameters?
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[*] posted on 7-6-2018 at 12:01


Quote: Originally posted by roXefeller  

If you want simple, go with acetone peroxide. Explosives aren't something we enter into looking for the simplest routes. You wouldn't jump out of an airplane with a kite just because it was easy to buy and parachutes were sold out. Get the tools, glassware, and the reagents that are necessary before jumping out the door. ETN was the very compound that started the "Life after detonation" thread.

And why are you scaling up your reaction when you're still working out the parameters?


Actually, the place where I am working does not have electricity and i cant bring electricity there too. Even if i bought the equipment i could not work with it.

Now i am scaling my reactions up cause yields are very good already and i did not have much ETN left over. Also i have plenty of reagents so I don't mind to scale it up a bit.
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Laboratory of Liptakov
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[*] posted on 8-6-2018 at 06:52


Haha....Parachutes were sold out... But : Explosives aren't something we enter into looking for the simplest routes. Truth,. Next: High yields?
Erythritol were dissolved in H2SO4 ? Works it ? Low temperature were used ? I am glad to hear it.....:-)....:cool:




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[*] posted on 23-12-2018 at 00:59
Erythritol Temp and How long it lasts


I have been experimenting for the last couple years on and off with ETN and I find the most productive way is to mix the acids first, then finally add the dry ground Erythritol. I let the temp get to around 25 degrees C. and nitrate for 30 minutes to 45 minutes with constant swirling. I found the higher temperatures do not reduce productivity efficiency. It seems to produce 140% (usually, or very close) yield before purifying. After purification the yield is a little over 75%, usually, sometimes greater. I rinse with sodium bicarbonate and water through the coffee filter and let dry. Then purify with Methyl Alcohol and pour the entire hot solution directly into a coffee filter and let drain into water again mixed with Sodium BiCarbonate. Let this sit at room temp, then place in fridge for 12 hours, re-filter and dry.

I have noticed even after deacidifying and washing numerous times and storing, the ETN turns to the tri-nitrate in about 1 year and a half, kept in a fridge and sealed well. The last day it exploded fully was around 16 months and on the 18th month it didn't do anything but fizzle. This was tested only with putting a small match head amount between aluminum foil and lighting with a torch. When at the 18th month it did not go off, I mixed a small portion of the degraded ETN into cold water and it dissolves. This makes me believe it lost some nitrogen and was not the tri-nitrate. I could be wrong, any help would be greatly appreciated.

I am a little disappointed that it does not have a better shelf life, although a year and a half is pretty good I guess. Anyone have any ideas to make it last longer? I was thinking of letting it sit in Ammonia water for an hour or so after my normal deacidification process. On the other hand, my Picric Acid lasts indefinitely, which I am very happy about.

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[*] posted on 23-12-2018 at 03:54


It sounds like your ETN had a pH that was off neutral ─ the final wash should be with a large volume of tepid water of strictly neutral pH...

Washing is something that can't be overdone.

My suspect would be slow alkaline hydrolysis?

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[*] posted on 23-12-2018 at 17:32


Thank you for the info! I will try what you say, unfortunately I won't know for another year and a half, but what you say does make sense. I don't believe I ever washed with just neutral PH water. My final wash was always with water mixed with sodium bicarbonate. I did not think the sodium bicarbonate would pose a problem as long as it was no longer acidic. I guess that is where I made my mistake? I am making a batch tonight, so hopefully I can get a batch that lasts indefinitely - or at least close, that is my goal. I would like to make quite a lot, then not have to make it for a few years or more. Thanks again!

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[*] posted on 24-12-2018 at 03:45


Quote:
I did not think the sodium bicarbonate would pose a problem as long as it was no longer acidic.

Bicarb. contamination is your culprit.

Its slow decomp.; 2NaHCO3 → Na2CO3 + CO2 + H2O significantly raises pH over time...

I've always used freshly distilled water (tap-water is full of shit) for the final wash ─ if left to stand its pH drops as CO2 absorbs and heating is required to bring pH back up to neutral.

Sobrero, early on, noted that NGl stored for 10 years gave an analysis close to the theoretical ─ and indeed most if not all organic nitrates may be stored indefinitely in the pure state.

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